US6217945B1 - Process for making multilayer coatings with a strippable topcoat - Google Patents

Process for making multilayer coatings with a strippable topcoat Download PDF

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Publication number
US6217945B1
US6217945B1 US09/269,094 US26909499A US6217945B1 US 6217945 B1 US6217945 B1 US 6217945B1 US 26909499 A US26909499 A US 26909499A US 6217945 B1 US6217945 B1 US 6217945B1
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polar material
process according
primer
top coat
substrate
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US09/269,094
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Michael Fowler
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PRC Desoto International Inc
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PRC Desoto International Inc
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Assigned to PRC-DESOTO INTERNATIONAL, INC. reassignment PRC-DESOTO INTERNATIONAL, INC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: FOWLER, MICHAEL
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/50—Multilayers
    • B05D7/56—Three layers or more
    • B05D7/58—No clear coat specified
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures

Definitions

  • This invention relates to the application to a substrate of a coating system in which a cured primer coating is overcoated with a top coat which is intended to be strippable, that is to say removable from the primed substrate by a stripping solvent without removal of the primer from the substrate.
  • a coating system in which a cured primer coating is overcoated with a top coat which is intended to be strippable, that is to say removable from the primed substrate by a stripping solvent without removal of the primer from the substrate.
  • Such coating systems are widely used on aircraft and may also be used on other substrates, for example commercial vehicles, cars, yachts or railway vehicles.
  • Aircraft are usually painted with a primer which is based on an epoxy resin and a curing agent, particularly an amino-functional curing agent, although the primer can be an alternative cured coating, for example polyurethane.
  • the top coat is usually based on polyurethane, particularly a polyester-urethane.
  • the coatings must resist water and certain organic solvents such as aviation fuel and preferably also resist hydraulic fluids based on phosphate esters such as tricresyl phosphate or tri-n-butyl phosphate, e.g. that sold under the trade mark “Skydrol”.
  • Each coating is generally cured by the reaction of components which have been packaged separately and are mixed at or shortly before application.
  • the top coat adheres to the primer so strongly that the top coat cannot be stripped without removing or at least damaging the primer.
  • Aircraft owners and operators would prefer a paint system in which the primer remained on the aircraft to prevent the stripping solvent contacting any resins, sealants or adhesives used in the aircraft construction or the metallic substrate and to avoid repeating the pre-treatment and primer coating of the aircraft.
  • GB-A-1511935 is a non-crosslinked polyamide. This at least partially resists the solvent used to remove the top coat and can itself easily be removed by alcohol-based solvents to reveal the primer.
  • DE-A-2528943 describes a linear non-crosslinked elastic polyurethane coating used between crosslinked polyurethane primer and top coat layers.
  • EP-A-147984 describes a barrier intermediate coating comprising a film-forming addition polymer comprising units of a vinyl aromatic monomer and units of a monomer containing a hydroxy alkyl group in an amount to provide a hydroxyl content of the addition polymer in the range 0.5 to 5 per cent by weight reacted with a polyisocyanate containing at least 2 isocyanate groups per molecule.
  • a non-volatile polar material is applied to the primed substrate from an aqueous liquid vehicle before coating with the top coat, the said polar material having sufficiently high affinity for the primer surface that it is not washed off the primer surface by water rinsing or by application of the top coat paint, whereby the said polar material facilitates the removal of the top coat from the primer by the stripping solvent.
  • the invention also provides a process for overcoating a substrate having a cured primer coating to facilitate the removal by a stripping solvent of a subsequently applied top coat, characterised in that a non-volatile acidic aromatic polar organic compound is applied to the primed substrate from aqueous solution, the said acidic aromatic compound having sufficiently high affinity for the primer surface that it is not washed off the primer surface by water rinsing.
  • a cured primer coating we mean a coating which is curable by chemical reaction when applied and which has cured sufficiently to be at least touch dry at the time when the polar organic compound (polar material) is applied.
  • the polar organic compound is thus usually applied at least 2 or 3 hours after the substrate has been primer coated and may be applied at any later time, including several days or more later when the primer is fully cured.
  • the polar material is not an intermediate coating as known from the prior art and is generally not a film-forming material. It is non-volatile, that is to say it does not evaporate to any significant extent at 20° C. In some instances it is preferably not polymeric, although polymers or oligomers having a plurality of anionic groups can be used and in other instances may be preferred.
  • the polar material particularly if it is not polymeric, may be applied at such a low thickness that it is present on the primer surface as a molecular monolayer or partial monolayer, for example a monolayer covering 10 to 60 or 80% of the surface area.
  • the polar material allows good adhesion between the top coat and the primer on application of the top coat and in service but greatly weakens the interlayer adhesion between the primer and the top coat when the top coat is swollen by stripping solvent.
  • the suitability of a candidate polar material can be readily assessed by applying it to the primed substrate and rinsing with water to see if it is completely removed.
  • the primer coating is preferably based on an epoxy resin cured with an amino-functional curing agent such as an amino-functional polyamide and/or an araliphatic diamine.
  • a crosslinked polyurethane primer is an alternative.
  • the primer generally contains an anticorrosive pigment such as a chromate, phosphate, phosphonate or molybdate and may contain one or more other pigments and/or fillers.
  • the primer coating can be applied from solution or dispersion in an organic solvent or can be a high solids or solventless composition or may be applied as an aqueous composition.
  • polar materials which have been found to be effective, particularly over amine-cured epoxy primers, contain at least one acidic group such as a carboxylic acid group or sulphonic acid or phosphonic acid group present in free acid or salt form.
  • carboxylic acid groups if present are preferably in free acid form whereas sulphonic or phosphonic acid groups if present are preferably fully or partially neutralised e.g. in alkali metal salt form.
  • the polar material is usually a polar organic compound, preferably a polar organic aromatic compound.
  • the acidic group is preferably attached directly to an aromatic ring.
  • Many of the effective compounds additionally contain at least one hydroxy group and/or amino group.
  • the polar material polar organic compound
  • the polar material preferably has a molecular weight in the range 120 or 150 up to about 1000 or 1500.
  • Many of the effective compounds are known as dyes, although one of the most preferred compounds is gallic acid (3,4,5-trihydroxy-benzoic acid), which is not generally regarded as a dye.
  • 2,5-Dihydroxybenzoic acid is also effective, although 3,5-dihydroxybenzoic acid is much less effective in giving stripping.
  • 4,5-Dihydroxy-1,3-benzenedisulphonic acid (generally used in disodium salt form) is also effective in giving selective stripping.
  • acidic dyes which have been found effective in giving selective stripping are Catechol Violet, Fast Green, Lissamine Green SF, Orange G, Amido Black and Methyl Orange. The chemical structures of these dyes are shown below.
  • polar materials can be used, for example mixtures of gallic acid with a dye such as Past Green.
  • acidic dyes which can give selective stripping are sulphonyl porphyrins, for example 5, 10, 15, 20-tetrakis (4-sulphonatophenyl)-porphine manganese (III) chloride of molecular weight 1023, bromocresol purple, calcion (a sulphonate-functional dye), fluorescent brightener 28 (an optical brightener), Nigrosin (Acid Black 2), Brilliant Black BN, citrazinic acid, xylenol blue Na salt, Reactive Blue 2, xylenol orange Na salt, Brilliant Blue R, Brilliant Blue G and chromoxane cyanine R.
  • Aurin (rosolic acid) which is an acid dye although it does not contain any carboxylic or stronger acid groups, is also moderately effective.
  • the dye Safranine O having the structure
  • acid-functional polymeric polar materials which have given selective stripping are a hyperbranched poly (5-hydroxyisophthalic acid), poly(styrene sulphonate) in sodium salt form, sodium polyphosphate and polyacrylic acid.
  • Guluronic acid oligomer and mannuronic acid oligomer obtained by depolymerisation of alginic acid are also effective. All of these materials can be applied from aqueous solution.
  • Gluconic acid is an example of a non-aromatic acidic organic polar compound which is quite effective in giving selective stripping. We have found that materials sold as surfactants are usually ineffective in giving selective stripping.
  • the concentration of polar material in the liquid aqueous vehicle applied to the primed substrate is generally in the range 0.0001 to 20 g/L (grams per liter).
  • the polar material is preferably applied from aqueous solution.
  • the aqueous composition is preferably coated on the primed substrate and then rinsed with water, although it may be simply coated on the primed substrate without rinsing.
  • the aqueous liquid vehicle may contain an organic solvent (preferably of low volatility) to improve wetting of the primer surface, for example a terpene (which may be used with a surfactant) or N-methyl pyrrolidone. If such an organic solvent is used it is preferably present at less than 20%, most preferably less than 10%, by weight of the aqueous liquid vehicle.
  • the aqueous solution of the polar material generally has a concentration of at least 0.01 g/L and preferably at least 0.1 g/L of the polar material, and the solution is preferably thickened, for example so that it is thixotropic or pseudoplastic or has a viscosity similar to that of conventional paints.
  • the thickening agent used can for example be a fine-particle silica gel such as that sold under the Trade Mark “Aerosil 200”, which can for example be used at 1 to 4% by weight of the aqueous composition, and/or a bentonite clay and/or a polysaccharide.
  • the concentration of polar material in such a thickened solution is generally up to 10 or 20 g/L, for example 0.2 to 5 g/L.
  • the aqueous composition can be applied by conventional coating methods such as spray, for example airless spray, roller or brush, and it is preferably left in contact with the primed surface for at least 1 or 2 minutes up to 1 or 3 hours or even 24 hours before rinsing with water.
  • spray for example airless spray, roller or brush
  • the aqueous solution of polar material is preferably applied to the primed substrate as a fine spray, for example an aerosol spray, to ensure even distribution of the polar material.
  • concentration of polar material in the aqueous solution is preferably 0.0001 to 2 g/L, particularly 0.001 to 0.01 or 0.1 g/L, for aerosol spray, although higher concentrations can be used if the aerosol spray is fine enough to give even distribution.
  • the amount of polar material applied is preferably 10 ⁇ 5 to 10 ⁇ 1 , most preferably 10 ⁇ 4 to 10 ⁇ 3 or 10 ⁇ 2 , grams per square meter if rinsing is not to be used.
  • This amount of polar material gives rise to a coating which is thicker than a monolayer and may be up to 50 molecular layers, for example 5 to 25 molecular layers, thick.
  • a partial monolayer generally gives the best results whereas for some dye molecules a coating thicker than a monolayer gives the best results.
  • the polar material should have sufficient affinity for the primer surface that it is not washed off the primer surface by water rinsing.
  • the top coat paint applied is generally a curable coating comprising two or three co-reactive components which are usually packaged separately and mixed at application (for example by twin-feed spray) or shortly before application (for example up to 8 hours before).
  • the top coat paint particularly for aircraft coatings, is preferably a polyurethane such as a polyester-urethane, although other curable paints such as polyester, fluoropolymer or acrylic polymer paints, based for example on oxazolidine-functional acrylic polymers, can be used.
  • the top coat paint is preferably applied from organic solvent solution, but it can in general be applied from dispersion in water and/or organic solvent.
  • the solution of polar material is preferably allowed to dry on the primed substrate for at least 30 minutes, preferably at least 2 or 3 hours, before the top coat is applied.
  • the top coat After the top coat has been allowed to cure, preferably for at least 3 days, it adheres firmly to the primer, and the coating system is resistant to spraying with salt-laden water and to immersion in “Skydrol” phosphate ester and generally to immersion in water without separation of the top coat from the primer or significant blistering.
  • the top coat is treated with a paint stripper in which it swells, particularly a stripper of a type used commercially to strip aircraft paints, swelling of the top coat is followed by detachment from the primer. The top coat lifts off the primer and may fall right away or is readily removed by low-pressure water washing.
  • the top coat can readily be removed within a time which is generally 10 minutes to 5 hours and usually 0.5 to 2 hours after application of the paint stripper, without any removal of the primer.
  • the primer may be somewhat swollen or discoloured by the paint stripper, but it resists removal with the top coat and continues to adhere to the substrate. Any swelling of the primer subsides as the paint stripper dries.
  • the stripper most widely used to strip aircraft paints, particularly polyurethane top coats is an aqueous thickened mixture of benzyl alcohol and formic acid.
  • Alternative strippers are alkaline thickened aqueous benzyl alcohol or a stripper based on methylene chloride and phenol (used to strip certain fluoropolymer and acrylic top coats).
  • the polar material bound to the primer surface when the paint stripper is applied. It is strongly preferred that the polar material should be re-applied to the primer surface before a fresh layer of top coat is applied so that the fresh top coat is strippable.
  • Aluminium panels were coated with a 20 micron layer of an epoxy primer based on a condensed bisphenol A/epichlorhydrin epoxy resin and an amine curing agent containing anticorrosive pigments applied from organic solvent solution and allowed to cure at ambient temperature.
  • the primed panels were sprayed with a 0.9 g/L aqueous solution of gallic acid. After 10 minutes the panels were rinsed with tap water and left to dry overnight. A partial monolayer of gallic acid adhered to the primer surface. Spectroscopic surface analysis indicated that the gallic acid monolayer covered about 15% of the surface and that the amount of gallic acid on the surface was about 3 ⁇ 10 ⁇ 5 g/m 2 of surface.
  • the panels were spray-coated with a pigmented polyurethane top coat paint at 60 microns dry film thickness applied from organic solvent blend.
  • the top coat was a 2-pack polyurethane of a type commonly used for aircraft, comprising a hydroxy-functional polyester component and an aliphatic polyisocyanate component. The top coat was allowed to cure under ambient conditions for two weeks before being tested for strippability and chemical resistance.
  • Some of the coated panels were coated with “Turco 9090” benzyl alcohol-based stripping solvent. After 90 minutes the top coat layer had lifted off the primer.
  • top coat was then readily removed by the low-pressure water wash used to clean off the stripping solvent (some fell off even before washing), leaving a clean intact primer surface.
  • Some of the coated panels were coated with “Turco 6776” formic acid-based stripping solvent. After 1 hour the top coat layer had lifted off the primer and was readily removed.
  • Example 1 The process of Example 1 was repeated using a 0.66 g/L solution of Fast Green dye in place of gallic acid. Spectroscopic surface analysis indicated that the dye monolayer covered about 35% of the surface and that there was about 1 ⁇ 10 ⁇ 4 g/m 2 of the dye on the surface. Example 1 was also repeated for both chemicals applied 19 hours (rather than 5 hours) after primer application. In all cases satisfactory stripping of the top coat was achieved (time required for clean strips may vary). The results are summarised in the following Table 1.
  • Example 1 and 2 were also tested for strippability using “Turco 1270/5” stripping solvent, which is an alkaline aqueous benzyl alcohol-based solvent.
  • the coating system of Example 2 gave a clean strip (clean lifting off the top coat) after 90 minutes.
  • the coating system of Example 1 required 4.5 hours in contact with the stripping solvent, but a clean strip of the top coat was then achieved.
  • the strippability test used was a quick test using formic acid. Very good strippability (top coat detached itself) was achieved in 10 minutes in Examples 5 and 6, and the top coat could be easily stripped off in Example 7 and fairly easily in Example 8.
  • Aluminium panels were chromic acid pickled prior to coating.
  • the primer specified in Table 2 below was spray applied and dried for 4 hours at 50% relative humidity (R.H.) and 22° C.
  • the primed panels were dipped in a 0.2% by weight solution of aqueous gallic acid for 20 minutes, then rinsed with tap water and air dried at 50% R.H. and 22° C. for 24 hours before topcoating with the top coat specified in Table 2. Stripping tests were carried out in duplicate, after 7 days' drying, on the fully coated panels at 50% R.H. and 22° C.
  • the strippers used were “Turco 9090” (formic/oxalic acid based) for Examples 9-14 and “Turco 5351” (methylene chloride/phenol based) for Examples 15-17. Two further dried panels were tested for Skydrol and water resistance (2 weeks' Skydrol immersion at 70° C. and 7 days' water immersion at 40° C.; respectively).
  • Examples 9 to 13 and 15 to 17 showed no deterioration in the Skydrol immersion test.
  • the paint system of Example 14 resisted Skydrol for 5 days but showed some loss of adhesion after 14 days' Skydrol immersion.
  • Aluminium panels were coated with an epoxy/amine primer clear coat as in Example 1 and aged for 4 hours at 23° C. before being dipped in a 1 g/L aqueous solution of the polar material at 30-35° C. for 30 minutes. The panels were not rinsed but were stood vertically to air-dry for 135 minutes, and then top-coated with Desothane white polyurethane top coat. The fully coated panel was dried at ambient temperature for about 24 hours and then at 40° C. overnight.
  • the time of contact in minutes with each stripping solvent is shown in Table 3, as is the degree of stripping, that is to say the percentage of the area of the panel over which the top coat was readily stripped from the primer.
  • Turco 9090 Turco 1270/5 % % Selec- Selec- Time of tive Time of tive Example Contact Strip- Contact Strip- No. Polar Material min ping min ping 18 Sulphonyl porphyrin 26 100 26 95 19 Hyperbranched 20 95 30 100 polyester of 5- hydroxy-isophthalic acid 20 Bromocresol purple 27 90 27 97.5 21 Calcion 27 100 27 95 22 Fast Green-Gallic 29 97.5 29 85 acid (50/50 by weight mixture) 23 Poly (styrene 25 90 25 100 sulphonate) Na salt 24 Guluronic acid 25 90 25 100 oligomer of Mn 520 25 Mannuronic acid 25 75 25 92.5 oligomer of Mn 2250 26 Fluorescent 27 90 57 92 Brightener 28 27 Brilliant Black BN 23 82.5 25 90 28 Sodium polyphosphate 25 75 44 95 29 4,5-dihydroxy-1,3- 35 80 48 85 benzene disulphonic acid, Na salt 30 Purpurogallin 25 60 25 100 31 Citrazinic acid 27

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Paints Or Removers (AREA)
  • Laminated Bodies (AREA)
  • Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
  • Formation Of Insulating Films (AREA)
  • Glass Compositions (AREA)
US09/269,094 1996-09-26 1997-09-24 Process for making multilayer coatings with a strippable topcoat Expired - Fee Related US6217945B1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
GBGB9620246.0A GB9620246D0 (en) 1996-09-26 1996-09-26 Improvements in or relating to coating substrates
GB9620246 1996-09-26
PCT/GB1997/002596 WO1998013148A1 (en) 1996-09-26 1997-09-24 Process for making multilayer coatings with a strippable topcoat

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EP (1) EP0930944B1 (es)
JP (1) JP2001500786A (es)
KR (1) KR20000036141A (es)
CN (1) CN1067301C (es)
AT (1) ATE200636T1 (es)
AU (1) AU734962B2 (es)
BR (1) BR9712129A (es)
CA (1) CA2271627A1 (es)
DE (1) DE69704628T2 (es)
ES (1) ES2158584T3 (es)
GB (1) GB9620246D0 (es)
NO (1) NO991462L (es)
PL (1) PL332373A1 (es)
TW (1) TW372201B (es)
WO (1) WO1998013148A1 (es)
ZA (1) ZA978599B (es)

Cited By (15)

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US6709697B1 (en) * 2002-10-15 2004-03-23 The United States Of America As Represented By The Secretary Of The Air Force Protective barrier coating for selective paint stripping processes
US20040244652A1 (en) * 2003-06-04 2004-12-09 Cameron Drake Starch-based abrasive absorbent
US20050288456A1 (en) * 2004-06-28 2005-12-29 Morkunas Bernard T Flexible, impact resistant primer
US20060004139A1 (en) * 2004-06-30 2006-01-05 Connelly Bruce A Polyurethane coatings with improved interlayer adhesion
US20060194705A1 (en) * 2005-02-28 2006-08-31 The Boeing Company Methods of applying cleaning solvent with titanate adhesion promoter to polymeric substrates
US20070054128A1 (en) * 2005-02-04 2007-03-08 Walker John A Multi-component epoxy-amine primer systems comprising a polythioether
US20100330372A1 (en) * 2007-05-17 2010-12-30 Johnsondiversey, Inc. Surface coating system and method
US20110036947A1 (en) * 2009-08-17 2011-02-17 Hexion Specialty Chemicals, Inc. Coating system for aircraft and aircraft coated therewith
US20130015292A1 (en) * 2011-07-12 2013-01-17 The Boeing Company Decorative Decal System for an Aircraft
US20160032149A1 (en) * 2014-07-31 2016-02-04 Gm Nameplate, Inc. Aerospace decal
US9868862B2 (en) 2011-05-25 2018-01-16 Diversey, Inc. Surface coating system and method of using surface coating system
US9909020B2 (en) 2005-01-21 2018-03-06 The Boeing Company Activation method using modifying agent
US10167546B2 (en) * 2015-04-29 2019-01-01 3M Innovative Properties Company Swellable film forming compositions and methods of nanoimprint lithography employing same
WO2019183669A1 (en) * 2018-03-26 2019-10-03 Commonwealth Scientific And Industrial Research Organisation Polymer coating compositions
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US8557386B2 (en) 2004-11-17 2013-10-15 Prc-Desoto International, Inc. Selectively strippable intermediate coatings and methods of use

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Cited By (21)

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US6709697B1 (en) * 2002-10-15 2004-03-23 The United States Of America As Represented By The Secretary Of The Air Force Protective barrier coating for selective paint stripping processes
US8815008B2 (en) * 2003-06-04 2014-08-26 Archer Daniels Midland Company Starch-based abrasive absorbent
US20040244652A1 (en) * 2003-06-04 2004-12-09 Cameron Drake Starch-based abrasive absorbent
US20050288456A1 (en) * 2004-06-28 2005-12-29 Morkunas Bernard T Flexible, impact resistant primer
US20060004139A1 (en) * 2004-06-30 2006-01-05 Connelly Bruce A Polyurethane coatings with improved interlayer adhesion
US10888896B2 (en) 2005-01-21 2021-01-12 The Boeing Company Activation method using modifying agent
US9909020B2 (en) 2005-01-21 2018-03-06 The Boeing Company Activation method using modifying agent
US20070054128A1 (en) * 2005-02-04 2007-03-08 Walker John A Multi-component epoxy-amine primer systems comprising a polythioether
US7498384B2 (en) 2005-02-04 2009-03-03 Ppg Industries Ohio, Inc. Multi-component epoxy-amine primer systems comprising a polythioether
US20060194705A1 (en) * 2005-02-28 2006-08-31 The Boeing Company Methods of applying cleaning solvent with titanate adhesion promoter to polymeric substrates
US7510773B2 (en) 2005-02-28 2009-03-31 The Boeing Company Methods of applying cleaning solvent with titanate adhesion promoter to polymeric substrates
US20100330372A1 (en) * 2007-05-17 2010-12-30 Johnsondiversey, Inc. Surface coating system and method
US20110036947A1 (en) * 2009-08-17 2011-02-17 Hexion Specialty Chemicals, Inc. Coating system for aircraft and aircraft coated therewith
US9868862B2 (en) 2011-05-25 2018-01-16 Diversey, Inc. Surface coating system and method of using surface coating system
US8986816B2 (en) * 2011-07-12 2015-03-24 The Boeing Company Decorative decal system for an aircraft
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US20160032149A1 (en) * 2014-07-31 2016-02-04 Gm Nameplate, Inc. Aerospace decal
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ZA978599B (en) 1998-03-26
TW372201B (en) 1999-10-21
EP0930944A1 (en) 1999-07-28
KR20000036141A (ko) 2000-06-26
NO991462L (no) 1999-05-19
PL332373A1 (en) 1999-09-13
CN1230908A (zh) 1999-10-06
ES2158584T3 (es) 2001-09-01
DE69704628D1 (de) 2001-05-23
JP2001500786A (ja) 2001-01-23
CA2271627A1 (en) 1998-04-02
AU4314397A (en) 1998-04-17
EP0930944B1 (en) 2001-04-18
BR9712129A (pt) 2000-01-18
GB9620246D0 (en) 1996-11-13
DE69704628T2 (de) 2001-09-13
AU734962B2 (en) 2001-06-28
WO1998013148A1 (en) 1998-04-02
NO991462D0 (no) 1999-03-25
CN1067301C (zh) 2001-06-20
ATE200636T1 (de) 2001-05-15

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